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ChemicalBook CAS DataBase List ethyl 2,3-diaMinobenzoate
37466-88-9

ethyl 2,3-diaMinobenzoate synthesis

2synthesis methods
61063-11-4 Synthesis
ethyl 2-amino-3-nitro-benzoate

61063-11-4
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Yield:37466-88-9 99%

Reaction Conditions:

with hydrogen;palladium 10% on activated carbon in ethyl acetate at 20; under 2585.81 Torr; for 30 h;

Steps:

7.II

Step II: 2,3-Diamino-benzoic acid ethyl ester (VIII); To a solution of compound (VII) (0.67 g, 0.00319 mol) in AcOEt (30 mL) was added Pd/C (10%) (0.05 g) and the mixture subjected to hydrogenation at 50 psi at room temperature for 30 hrs (TLC monitoring: cyclohexane/AcOEt 2:1). The mixture was filtered and concentrated under reduced pressure to give the compound (VIII) (0.57 g) as a light brown solid, m.p. 56-57°C. Yield: 99%. [1H] NMR (400 MHz, CDCl3, δ): 1.38 (t, J=7.1Hz, 3H, OCH2CTf5), 4.30 (bs, 4H, NH2), 4.33 (q, J=7.1Hz, 2H, OCH2CH3), 6.60 (dd, J=8.2Hz, 7.6Hz, IH) 6.84 (d, J=7.6Hz, IH) 7.49 (d, J=8.2Hz, IH) (aromatic protons).

References:

WO2008/12852,2008,A1 Location in patent:Page/Page column 25; 38-39